Manufacture of pigment colors



Patented May 17, 1932 r STATES CARL IMMERHEISER 'AND BODO ZSCI-IiI/IMER,or] LUnwIesHarENpN-mHEmnmE,

GER-MANY, ASSIGNORS, BY MESNE ASSIGNMENTfi TO -a GENERALVANTLINEWOIRKSJ:me, or NEW YORK, N. Y., A CORPORATION or DELAWARE." V I a Y 1MANUFACTURE onrrennnrcotons I in) Drawing. Application filed April 22, 192e ,'seria1n 103,966, and in -Germany 1, i925.

In the Patent No.1,529,891there is'described aprocess for themanufacture of 1 green pigment colors by acting onnitrosobeta-naphthol,preferably in the 'form of its 5 bisulfite compound, with ironsalts inthe presence or absence of substrates.

We have now found that the shade of the said pigment colors, Whileretaining or even increasing their excellent fastness to light andalkalies, can be influenced by preparing the said green pigment color inthe presence of basic dyestuffs, preferably those belonging to themalachite green series. The process may be carried out for example bydissolving the nitroso-beta-naphthol in Water with the aid of abisulfite, adding the iron salt in the manner described in the PatentNo. 1,529,891 or in any other manner or in molecular proportions forexample. in a still lnuch more restricted quantity, or in largeramounts, for instance in the proportion of about 1 atom of iron to twomolecules of nitroso-beta-naphthol in the absence or pres ence of Turkeyred oil or other dispersing agents, adding the basic dyestuff to themixture and precipitatingthe pigment color by means of an alkalineagent, for example sodium carbonate. It has been proved of specialadvantage to add a small quantity of the alkaline agent insufiicient forprecipitation before adding the basic dyestuff and then precipitatingthe pigment by adding the rest of the alkaline compound.

Instead of nitroso-beta-naphthol, its bisulfite compound may also beemployechpreferably with an addition of some excess of hisulfitesolution.

Theproducts obtained bythe process. ac-

cording to the present invention are faster at to light than a meremechanical mixture of the iron compound of alpha-nitroso-betanaphtholwith a basic dyestufl'. They are therefore thought to be a kind ofcomplex compound, but applicantsdo not Wish to bind "*45 themselves tothis expl n 7 F V 1116 partsof alpha-nitroso-betarnaphthol '-'.'WhatWec-laim'is: f 1. The process of manufacturing pigment means-ofanalkaline-agentx' paste of 15'per cent strength that is about 167-parts of alpha-nitroso-beta-naphthol are mixed Wltl1'650 parts of sodium'bisulfite solution of 38 BS a-nd 3000'parts of Water and dissolved bystirring for 3 hours. 'The -tb 7 solution is filteredan'd' filled upvvithWater to about 5000 parts. 48 parts of crystallized ferrous sulfatedissolved in 960 parts 'of Water 24 parts of Turkey red oil in 24O'partsp of wa'ter, 100 parts of soda ash clissolved-in""' 1000 parts of Waterand 40 parts of diamond greenBX (see color index No. 657) dissolved 'in4000 parts 'of tvater are then added'toithe solution ;one aftertheothernwhereupon a Y solution of 260 parts of soda ash-in 26O0 -parts 6B'of water is caused to run in slowly.- 1 After "the greenfp'igment coloris completely "precipitated, 4 parts of aluminium lhydroxid in the formof a4 percentflpaste are added;f,the

product is Washed by decanting twice With Water and filtered 0H. About1'12O parts' of the pigment color'in' the form of a l2 per-cent pasteare obtained. "The color possesses 'ex- I cellent fastness to light'andjlime.

colors which comprises-acting with aniiron salt on nitroso beta''naphthol -i'n the presence of a basicdyestuff and precipitating-the pig- 2. The process'of manufacturing pigment colors Which comprises actingwith an 113011 salt on nitroso-beta-naphthol in the j prese nce of abasic dyestulfand a substrate and precipitating thepigment color bymeansjof an alkaline agent.

r 3. The process of manufacturing pigment 7 colors Wlnch comprls'es'acting wv-itlran rro'n salt on nltroso-beta-naphtholj1nthe presenceofa'basie'dyestuff'and a'dispersingagentland precipitating' the pigmentcolor means; of an alkaline agent. p v

p 4. The process of manufacturing pigment V colors-"Which comprisesmixingfan iron salt solution {with a solution of nitroso betanaphthol ina Water solutionofa bisulfite,

adding an alkaline agent in aquantity'insuifi V cien't' forprecipitation, adding a basicd y'estuff and precipitating thepi gmentcolor 'by Qcomplex composition of an iron compound ofnitroso-betanaphthol and a basic dyestufi', v40

; alkaline. agent.

5. The process of manufacturing pigment cipitating the pigment color bymeans of an colors which comprises acting with an iron alkaline agent.

salt on nitroso-beta-naphthol in the presence of a basic dyestulf of themalachite green series, and precipitating the pigment color by means ofan alkaline agent. V

6. The process of manufacturing pigment colors which comprises actingwith an iron 'salt on nitroso beta-naphthol in the presence of diamondgreen BX and precipitating the pigment color by means of an alkalineagent.

7 The process of manufacturing pigment colors which comprises mixing aniron salt solution with a solution of nitroso-betanaphthol in abisulphite, adding an alkaline agent ina quantity insuflici-ent forprecipitation, adding a basic ldyestuff of the malachite green series,and precipitating the pigment color by means of an alkaline agent.

.8. The process of manufacturing plgment colors which comprises mixingan iron salt solution with a solution of nitroso-betanaphthol in abisulphite, adding an alkaline agent in a quantity insufficient forprecipitation, adding diamond green BX, and precipitating the pigmentcolor by means of an 9. The process of manufacturing pigment Jcolorswhich comprises mixing a solution of about 48 parts of ferrous sulfatewith a solution of about 167 parts of nitroso-betanaphthol in abisulphite, adding an alkaline agent inaquantity insufficient forprecipita- In testimony whereof we have hereunto set our hands.

tion,- adding aboutLO parts of diamond green BX, and precipitating thepigment color by *means of an alkaline agent.

10. Asa new article of manufacture, a

which composition is faster tolight than the mere mechanical mixture ofthe said two components, and which is obtained by acting a withan ironsalt on nitroso-beta-naphthol in the presence of a basic dyestuff, andprecipitating the pigment color by means of an alkaline agent.

,1 1. As a, new article of manufacture, a complex compositlon of anlroncompound of nitroso-beta-naphthol anda basic dyestuif of thelnalachite'green series. which com-position is faster to light than themere mechanical mlxture of the said two components, and which isobtained by acting with an iron salt of an alkaline agent. l 12. As anew artlcleof manufacture, a

complex composition of an iron compound of nitroso-beta-naphthol anddiamond green BX, which composition is faster to light than the meremechanical mixture of the said two components, and which is obtained byacting with an iron salt on nitroso-beta-naphtholin the presence ofdiamond green BX, andpre-

